Continuous two zone treatment of fibrous materials with water-tierce solvent and hydrocarbon-tierce solvent mixture



3,390,950 TERIALS TIERCE July 2, 1968 A. DELFORGE CONTINUOUS TWO ZONETREATMENT OF FIBROUS MA WITH WATER-TIERCE S VENT AND HYDROCARBON- ENTMIXTURE Filed March 19654` 2 Sheets-Sheet 1 www CONTINUOUS TWO ZONETREATMENT OF FIBROUS MATERIALS July 2, 1968 A. DELFCRG'E 3,390,950' lWITH WATER-TIERCE.' SOLVENT AND HYDROCARBON--TIERCE SOLVENT MIXTUREFiled March 9. 1964 2 Shee'f.s'r`hee\`I 2 United States Patent O 3 7Claims. (cris-139.1)

This invention relates to a method for treating fibrous material, inwhich the material is treated on a foraminate conveyor belt with water,with a hydrocarbon solvent with strong 4extracting power, and with atierce solvent which mixes partly with water and partly with thehydrocarbon solvent.

Such a method is disclosed in the instant inventors U.S. Patent No.3,210,148 has been inserted in vits place.

This previous method pertains particularly to the treatment of wool,while the present invention relates to the treatment of fibrousmaterials in general and thus among others to the treatment of Wool.

`According to said known method, the material to be treated is-sprinkledin defined zones, separately with water, with a tierce solvent thatmixes partly with Water and partly with a hydrocarbon solvent, and nallywith this hydrocarbon solvent.

According to this application, the purpose is to provide avmethod whichis simpler and reduced to two steps of treatment. On the other hand, theinvention has for its object to provide a method which may be worked bymeans of an uncomplex installation. The invention has also for itsobject to provide a method that insures aA fast and deep application ofthe various liquids used.

VFor this purpose, the treatment is essentially made in two zones, theliquids which have passed through the material being collected in thesame decanting tank, the lower phase being returned at least partly overthe material in the rst zone, the upper phase bein-g returned at leastpartially above the second zone.

ln an advantageous embodiment of the invention, the material is treatedin the second zone with the upper phase in counter-current combined withclosed-circuit circulations.

In a particular embodiment of the invention, one adds extracted productto the upper phase which is supplied to the closed circuit which isprovided nearest the discharge side of the conveyor.

The invention also relates to an installation for working the abovemethod.

In this connection, the invention relates to an installation` fortreating brous materials whichl comprises a foraminate conveying belt,sprinklers above the conveyor and a decanting tank underneath theconveyor.

Such an installation is already known from the above U.S. patent.However, in said known installation, it is but a part of the upper phaseof the liquids collected in the decanting tank which may be returnedabove the conveyor to be used there together with alcohol supplied fromthe outside, for the intermediate treatment between the water treatmentand the hydrocarbon solvent treatment.

The invention according to the present application however enables acomplete treatment of the brous material by means of the liquidscollected in the decanting tank the phases of these liquids beingdischarged only to recover materials which -have been extracted from thewool.

For this purpose, sprinklers above a first zone of the conveyor areconnected to a sucking opening which is ice located in the lower part ofthe tank, while sprinklers above a second zone of the conveyor areconnected to a sucking opening in the upper part of the tank.

In a preferred embodiment of the invention, the installation comprises adecanting tank which is divided into compartments by partitions thatform overflows and which extend to some distance from the bottom so asto have a passage between the bottom and each partition.

In a particular embodiment of the invention, each compartment isprovided with a sucking opening which is located in the upper parttheerof and which is connected, through a pump and a pipe, to at leastone sprinkler which is provided above the collecting vessel whichsupplies .this same compartment.

Other details and features of the invention Will stand out from thedescription given below by way of non limitative example and withreference to the accompanying drawings, in which the single figure(divided in FIG- URES la and lb) shows diagrammatically an installationfor treating brous material according to the invention.

The invention shown in the figure comprises an endless conveyor withforaminate belt 1, which is guided at the ends by two drums (not shown),one of said drums only ,guiding the conveyor while the other one guidesand drives said conveyor.

Through the pipe 2, Water or a diluted alcohol solution in water isbrought to the sprinkler 3, which is located on the loading side for thefibrous material to be treated. This material is for instance wool. Forthe ease of the explanation, this material is called wool hereinafter,but it must be understood that the invention also applies to thetreatment of other fibrous materials. The hopper that brings the woolabove the conveyor has not been shown, the wool is brought on the belt-1 adjacent the pipe 2 and it moves together with the upper side of theconveyor along the direction of arrow 4. The freshlyentered wool is thusfirst rof all sprinkled with the liquid supplied by the pipe 2, whichleads to the sprinkler 3. The output of the sprinkler 3 is regulated bya valve 5. In the feeding `direction of the wool, the sprinkler 3 isfollowed by sprinklers 6 the output of which is regulated by valve 7 andto which is supplied liquid forced by a pump 8 into the outlet pipe 9thereof. The pump 8 sucks through a pipe 10, which is connected in turnto a sucking opening 11, the lower phase that forms in the decantingtank 12.

As results from the description given hereinbelow, the various liquidswhich have passed through the wool are nally collected throughcollecting vessels 13 and pipes 14, into one and the same decanting tank12. These liquids are essentially comprised of the aqueous alcoholsolution which is supplied by the pipes 2 and 15 and of a solution whichis rich in hexane and which is introduced into the installation throughthe pipe 16. These various liquids which are circulated as explainedlhereinbelow, finally take along into the decanting tank the materialswhich have been extracted from the wool, such as greases and siint, aswell as the impurities which are taken physically a ong.

The liquids collected in the decanting tank do actually decant veryrapidly in two quite different phases which are separated by anintermediate layer. This separating.

water. The upper phase is thus hexane-rich and poor in isopropylalcohol; due to this phase containing practically hexane, it does form amicella rich in grease. This upper phase is designated by reference 17.The lower phase 18 is an aqueous alcohol solution and comprisesessentially the salts and notably those potassium salts which areWater-soluble. An intermediate layer 19 comprises notably the mucilagesand forms a defined separation between the clear upper phase,hexane-rich, and the muddy lower phase, which is essentially comprisedof an aqueous alcohol solution.

A dragging chain 20, guided by the drums 21, is driven along thedirection of arrows 22. On that side where the wool leaves the endlessconveyor 1, the bottom of the decanting tank 12 is provided with aslanting part 23 the upwards gradient of which corresponds to thefeeding direction of the lower side of the dragging chain 20. The sandsand other solid materials comprised in the lower phase 18 are takenalong by the chain 20 and fall into the pipe 24 which discharges themfrom the installation.

In the feeding direction of the conveyor 1, that is along the directionof arrow 4, the sprinklers 6 are followed by a sprinkler 25 which issupplied by the pipe 15, a valve 26 regulating the liquid flow ratethrough the sprinkler 25. As stated above, the pipe supplies through thesprinkler an alcohol-richsolution. Water and alcohol are thus introducedin the installation through the pipes 2 and 15.

Still lalong the direction of arrow 4, the sprinkler 25 is followed bytwo pressing rollers 27, one of which lies underneath and the other oneabove the upper side of the conveyor; the wool is thus freed from thelarger part of the liquid by passing through the pressing rollers 27.The wool then passes below a series of sprinklers 28. Each sprinkler 28is connected by a pipe 29 to the outlet of a pump 30. Each one of thepumps 30 is supplied with the upper phase 17 of the liquids collected inthe decanting tank 12 through a sucking opening 31 and a sucking pipe32. A valve 33 arranged in pipe 29 allows to regulate the output. Thesucking openings 31 are located in the upper part of the tank 12somewhat below the level which is normally reached by the liquids in thetank. The sprinklers 28 thus bring the upper phase 17 formed in thedecanting tank 12 above the wool. The wool is thus sprinkled with ahexane-rich micella.

While the micellae sent to the various sprinklers 28 come from the samedecanting tank, they however do not have identical compositions. Indeedthe decanting tank 12 is divided in various compartments by partitions34. The height of these partitions is such as to allow the overflowingfrom one compartment to another. On the other hand, these partitions 34do not reach down to the bottom 35 of the decanting tank 12. The lowerphase 18, formed in the decanting tank 12, may thus pass from onecompartment to another without being constricted by the partitions 34;the space left free between the lower edge of the partitions 34 and thebottom 35 of the decanting tank 12 is also necessary to let the lowerside of the dragging chain 20 pass through. The various partitions 34are provided with an ejector 36 at the level of the intermediate layer19 which separates the upper phase 17 from the lower phase 18. Theejectors 36 are thus essentially provided to advance the intermediatelayer 19 along the feeding direction of the lower side of the draggingchain 20. Each ejector 36 is connected by a pipe 37 in which is arrangeda valve 38, to a pipe 29 which is supplied by a sucking opening 31located on the opposite side of the partition 34. Opening of the valve38 t'nus causes advancing of the intermediate layer 19 along the feedingdirection of the lower side of the dragging chain 20 by means of aliquid stream which is comprised of the upper phase 17, said liquidhowever entering the same compartment wherefrom it was sucked by thesucking opening 31. The ejectors 36 thus do not inuence in principle themovement oi the upper phase from one compartment to another of thedecanting tank.

A partition 39 separates the last one of the compartments connectedthrough a sucking opening 31, pipes 32 and 29 and a pump 30, to asprinkler 28, from a compartment 40 which is located on the dischargeside of the conveyor 1. The compartment 40 is supplied with the lowerphase from the compartment adjacent the loading side, through the'opening 41 which is left free between the' bottom 35 of the tank 12 andthe partition 39. On the other hand, the compartment 40 vis suppliedwith hexane-rich solution by the pipe 16 through an ejector 42 whichsupplies at the same time the compartment 40 with the intermediate layerfrom said adjacent compartment. A valve 43 regulates the liquid ow ratesupplied by the pipe 16 through the ejector 42 into the compartment 40.The liquid supplied through the pipe 16 comes from a refining anddistilling installation which comprises a unit with the installationshown.

The compartment 40 thus receiving a hexane-rich solution, as well as thecomponents of the lower'phase and of the intermediate layer of thepreceding compartments of the decanting tank, in this compartment isformed a lower phase 45, an intermediate layer 46 and an upper phase 44.A sucking opening 47, a pipe 48, a pump 49 and a pipe 50 bring the upperphase formed in the compartment 40 into the adjacent compartment whichis located on the loading side of the conveyor. This last compartmentthus receives in the upper part thereof a hexane-rich solution whichcomprises about 13% alcohol, but which is nearly substantially free ofgrease and other materials to be extracted from the wool. The suckingopening 31 of this compartment brings this upper phase above the woollwhich lies above that collecting' vessel 13 which is nearest thedischarge side of the conveyor. The liquid coming out ofthe sprinklers28 that are present above that collecting vessel'13 nearest thedischarge end of the conveyor, passes through the wool layer and it iscollected in said collecting vessel. A pipe 14 brings the liquidcollected in this collecting vessel to the compartment 51 of thedecanting tank 12. Part of the liquid collected in the compartment 51overilows above the partition 34 which bounds it on the loading side ofthe conveyor into the adjacent compartment 53 which is located on theloading side of the conveyor. Thus each one of the compartments 51, 52,53, 54 and 55 overflows above that partition 34 which bounds it on theloading side of the conveyor into that compartment 52, 53, 54, 55 and 56which is located on the loading side of the conveyor. There thus occursthrough the decanting tank 12 a ow of upper phase 17 in the directionopposite the feeding direction of the upper side of the conveyor. At thesame time, the liquid upper phase from each compartment is returnedthrough a sucking opening 31, a pipe 32, a pump 30, a pipe 29 andsprinklers 28, above the collecting vessel 13 which supplies this samecompartment through -a pipe 14.

Circulating of the kupper phase with a large ow is thus produced foreach one of the compartments 51 to 56, while at the same time there isproduced a somewhat more restricted flow from the compartment 51 towardscompartment 56 through compartments 52 to 55.

Each series of sprinklers 28 supplied from the same compartment isfollowed by pressing rollers 27, in such a way that the wool be freedfrom the largest part of the liquid thereof before passing to the zonecovered by the sprinklers 28 nearer the discharge side of the conveyor.

As described above, pressing rollers 27 are also provided between thesprinkler 25 and the sprinklers 28 that correspond to compartment 56.

The wool fed to the upper side of the `conveyor 1 is thus sprinkled bythe sprinklers 3, 6 and 25 with an aqueous alcohol solution which iscomprised at least partly of the lower phase which forms in thedecanting tank 12. Thereafter, the wool is sprinkled with a hexane-richsolution which is comprised of the upper phase formed in the decantingtank.

The intermediate layer 46 and the lower phase 45 of the compartment 40are discharged through the pipes 57 and 58 to an installation fordistilling the muds for-med by this lower phase 45 and this intermediatelayer 46. For this purpose, the pipe 57 is connected to a suckingopening 59 that lies at the level of the intermediate layer 46, whilethe pipe 58 is connected to a sucking opening 60 which is located at thelevel of the lower phase 45. A valve 61 is arranged in the pipe 57 and avalve 62 in the pipe 58.

The lower part of the decanting tank 12 also communi- Cates by anopening 63 with a compartment 64 which is separated from the tank properby the partition 65- and serves as florentine. The opening 63 is locatedin the lower part of the tank 12 and of the compartment 64, in such away that only the lower phase 18 may enter the compartment 64 throughthe opening 63. The compartment `64 overflows into the pipe 66 whichleads to the installation for distilling the muds, mentioned above. Avalve 67 allows to regulate said discharge.

The grease-rich micella comprised of the upper phase from thecompartment 56 is sucked through the sucking opening 68 which leads by apipe 69, in which is arranged a valve 70, towards an installation fordistilling micella. However, part of the liquid supplied by the pipe 69may be returned through the pipe 71 into the compartment 51. A valve 72allows to regulate the rich micella flow which is sent towards thecompartment 51 of the decanting tank 12, while an output-meter 73`enables to control this flow. This recycling of rich micella adds greaseto the micella of the compartment 51 which is sent on the wool on thedischarge side, in such a way that the amount of grease in the wool isadjustable. Indeed, the cleaning of the wool by means of the micella asdescribed above would normally give a wool which is too poor in greaseand consequently a frangible fiber. This drawback is avoided by makingthe micella richer in the last compartment.

From the above description, there results that a hexane-rich solutionfrom the distilling installation is supplied to the installation throughthe pipe 16. This micella gives an upper phase which is substantiallyfree from grease in the compartment 40 and it is brought by the pipe 50into the compartment 51. By passing through the various circuits and invarious locations through the wool layer, this micella gets richer andpasses from compartment to compartment in the direction of the loadingside of the conveyor, finally to leave the installation, after gettingricher in grease, through the pipe 69 towards the distillinginstallation for the grease-rich micella. On the other hand, the aqueousalcohol solution which is supplied to the installation through the pipes2 and 15 leaves this installation through the pipes 66, 57 and 58towards a mud distilling installation. The aqueous alcohol solution,freed from the solids and the salts, which comes from the mud distillinginstallation, is introduced again in the installation as shown in theligure, through the pipe 15. Thus, the wool is essentially treated in arst zone with an aqueous alcohol solution and in a second zone with ahexane-rich solution. The sprinklers 3, 6 and 25 determine the Iirstzone. The sprinklers 28 determine the second zone.

After these sprinkling zones, the upper side of the conveyor 1 passesthrough zones 'for evaporating the solvent, for eliminating the solventgases and for conditioning, as already known from the above U.S. patent.

It must be understood that the invention is in no way limited to theabove embodiments and that many changes may be brought therein, withoutdeparting from the scope of the invention as dened by the appendedclaims.

I claim:

1. Method for treating brous material, in which the material is treatedon a forarninate conveyor belt with water, with a hydrocarbon solventwith stron-g extracting power, and with a tierce solvent which mixespartly with water and partly with the hydrocarbon sol-vent, whichfurther comprises making the treatment essentially in two zones, theliquids which have passed through the material being collected in thesame decanting tank, the lower phase being returned at least partly overthe material in the -rst zone, the upper phase being returned at leastpartially above the second zone.

2. Method as claimed in claim 1, in which the material is treated in thesecond zone with the upper phase in countercurrent combined withclosed-circuit circulations.

3. Method as claimed in claim 2, in which one adds extracted product tothe upper phase which is supplied to the closed circuit which isprovided nearest the discharge side of the conveyor.

`4. Method as claimed in claim 1, in which htere is caused in thedecanting tank a movement of the upper phase in the direction oppositethe feeding direction of the conveyor, while a movement of theintermediate layer is caused in the feeding direction of the conveyor.

5. Method as claimed in claim 4, in which there is caused in thedecanting tank a movement of the lower phase in the feeding direction ofthe conveyor.

6. Method as claimed in claim 4, in which from the decanting tank aretaken the lower phase and the upper phase which are subjected separatelyto distilling and returned above the conveyor.

7. Method as claimed in claim `6, in which the distilled upper phase isreturned above the conveyor through the decanting tank.

References Cited UNITED STATES PATENTS 163,729 5/1875 Braun 8-139.1899,339 9/ 1908 Schuman 8-139.1 1,527,369 2/1925 Meyer 8--139.13,210,148 10/ 1965 Delforge 8--139.1

FOREIGN PATENTS 763,657 12/ 1956 Great Britain. 231,557 11/1960Australia.

NORMAN G. TORCHIN, .Primary Examiner.

I. C. CANNON, Assistant Examiner.

1. METHOD FOR TREATING FIBROUS MATERIAL, IN WHICH THE MATERIAL ISTREATED ON A FORAMINATE CONVEYOR BELT WITH WATER, WITH AHYDROCARBONSOLVENT WITH STRONG EXTRACTING POWER, AND WITH A TIERCE SOLVENT WHICHMIXES PARTLY WITH WATER AND PARTLY WITH A HYDROCARBON SOLVENT, WHICHFURTHER COMPRISES MAKING THE TREATMENT ESSENTIALLY IN TWO ZONES, THELIQUIDS WHICH HAVE PASSED THROUGH THE MATERIAL BEING COLLECTED IN THESAME DECANTING TANK, THE LOWER PHASE BEING RETURNED AT LEAST PARTLY OVERTHE MATERIAL IN THE FIRST ZONE, THE UPPER PHASE BEING RETURNED AT LEASTPARTIALLY ABOVE THE SECOND ZONE.